#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:00:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179088 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/50/4305055.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4305055
loop_
_publ_author_name
'Chaitali Biswas'
'Michael G. B. Drew'
'Ashutosh Ghosh'
_publ_section_title
;
Stabilization of a Helical Water Chain in a Metal-Organic Host of a
Trinuclear Schiff Base Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4513
_journal_page_last               4519
_journal_paper_doi               10.1021/ic8002542
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C22 H38 Cu2 N8 Ni O4'
_chemical_formula_weight         664.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.481(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9546(10)
_cell_length_b                   16.0561(19)
_cell_length_c                   10.4613(12)
_cell_measurement_temperature    150(2)
_cell_volume                     1442.3(3)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_sigmaI/netI    0.2802
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6468
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    2.148
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.752
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3972
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.752
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0609P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                1545
_reflns_number_total             3972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8002542-file003_2.cif
_cod_data_source_block           3
_cod_database_code               4305055
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0910(6) 0.6016(3) 0.5664(5) 0.0249(12) Uani 1 1 d . . .
C2 C 0.1422(6) 0.4845(3) 0.4029(5) 0.0218(11) Uani 1 1 d . . .
C12 C 0.6086(5) 0.5748(3) 0.2724(5) 0.0227(12) Uani 1 1 d . . .
C13 C 0.6826(6) 0.5326(3) 0.1926(5) 0.0261(12) Uani 1 1 d . . .
H13 H 0.7666 0.5594 0.1748 0.031 Uiso 1 1 calc R . .
C14 C 0.6436(5) 0.4525(3) 0.1348(5) 0.0206(11) Uani 1 1 d . . .
C16 C 0.5049(6) 0.3221(3) 0.1006(5) 0.0260(12) Uani 1 1 d . . .
H16A H 0.6026 0.2956 0.1017 0.031 Uiso 1 1 calc R . .
H16B H 0.4404 0.3252 0.0089 0.031 Uiso 1 1 calc R . .
C17 C 0.4235(6) 0.2728(3) 0.1831(5) 0.0246(12) Uani 1 1 d . . .
H17A H 0.3797 0.2226 0.1356 0.030 Uiso 1 1 calc R . .
H17B H 0.4980 0.2566 0.2663 0.030 Uiso 1 1 calc R . .
C121 C 0.6666(6) 0.6592(3) 0.3232(5) 0.0308(13) Uiso 1 1 d . . .
H12A H 0.5801 0.6939 0.3253 0.046 Uiso 1 1 calc R . .
H12B H 0.7209 0.6836 0.2654 0.046 Uiso 1 1 calc R . .
H12C H 0.7362 0.6543 0.4115 0.046 Uiso 1 1 calc R . .
C141 C 0.7398(6) 0.4211(3) 0.0475(5) 0.0297(13) Uani 1 1 d . . .
H14A H 0.8021 0.3748 0.0902 0.045 Uiso 1 1 calc R . .
H14B H 0.8065 0.4649 0.0336 0.045 Uiso 1 1 calc R . .
H14C H 0.6720 0.4036 -0.0368 0.045 Uiso 1 1 calc R . .
C181 C 0.1671(7) 0.3366(3) 0.0881(5) 0.0376(14) Uani 1 1 d . . .
H18A H 0.1284 0.2836 0.0507 0.056 Uiso 1 1 calc R . .
H18B H 0.2048 0.3674 0.0249 0.056 Uiso 1 1 calc R . .
H18C H 0.0847 0.3672 0.1086 0.056 Uiso 1 1 calc R . .
C182 C 0.2390(6) 0.2774(3) 0.3106(5) 0.0298(13) Uani 1 1 d . . .
H18D H 0.1478 0.3043 0.3218 0.045 Uiso 1 1 calc R . .
H18E H 0.3185 0.2763 0.3944 0.045 Uiso 1 1 calc R . .
H18F H 0.2135 0.2214 0.2798 0.045 Uiso 1 1 calc R . .
O11 O 0.4911(4) 0.54731(19) 0.3070(3) 0.0258(8) Uani 1 1 d . . .
O100 O 0.5508(4) 0.3753(2) 0.4668(3) 0.0233(8) Uani 1 1 d D . .
H1 H 0.548(4) 0.407(2) 0.5310(17) 0.028 Uiso 1 1 d D . .
H2 H 0.640(4) 0.371(3) 0.460(3) 0.028 Uiso 1 1 d D . .
Cu1 Cu 0.40189(7) 0.43687(4) 0.27047(6) 0.02135(19) Uani 1 1 d D . .
Ni2 Ni 0.0000 0.5000 0.5000 0.0223(2) Uani 1 2 d S . .
N1 N 0.1495(5) 0.6649(3) 0.6077(4) 0.0305(11) Uani 1 1 d . . .
N2 N 0.2327(5) 0.4721(3) 0.3446(4) 0.0253(10) Uani 1 1 d . . .
N15 N 0.5342(5) 0.4069(2) 0.1586(4) 0.0213(9) Uani 1 1 d . . .
N18 N 0.2961(4) 0.3238(2) 0.2117(4) 0.0215(9) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 Ni2 179.3(4) . . ?
N2 C2 Ni2 177.6(5) . . ?
O11 C12 C13 125.0(5) . . ?
O11 C12 C121 116.2(4) . . ?
C13 C12 C121 118.8(4) . . ?
C12 C13 C14 126.7(5) . . ?
C12 C13 H13 116.6 . . ?
C14 C13 H13 116.6 . . ?
N15 C14 C13 122.3(4) . . ?
N15 C14 C141 121.1(5) . . ?
C13 C14 C141 116.5(4) . . ?
N15 C16 C17 107.8(4) . . ?
N15 C16 H16A 110.1 . . ?
C17 C16 H16A 110.1 . . ?
N15 C16 H16B 110.1 . . ?
C17 C16 H16B 110.1 . . ?
H16A C16 H16B 108.5 . . ?
N18 C17 C16 110.3(4) . . ?
N18 C17 H17A 109.6 . . ?
C16 C17 H17A 109.6 . . ?
N18 C17 H17B 109.6 . . ?
C16 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C12 C121 H12A 109.5 . . ?
C12 C121 H12B 109.5 . . ?
H12A C121 H12B 109.5 . . ?
C12 C121 H12C 109.5 . . ?
H12A C121 H12C 109.5 . . ?
H12B C121 H12C 109.5 . . ?
C14 C141 H14A 109.5 . . ?
C14 C141 H14B 109.5 . . ?
H14A C141 H14B 109.5 . . ?
C14 C141 H14C 109.5 . . ?
H14A C141 H14C 109.5 . . ?
H14B C141 H14C 109.5 . . ?
N18 C181 H18A 109.5 . . ?
N18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
N18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
N18 C182 H18D 109.5 . . ?
N18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
N18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C12 O11 Cu1 125.8(3) . . ?
Cu1 O100 H1 107.9(17) . . ?
Cu1 O100 H2 106.2(19) . . ?
H1 O100 H2 112(3) . . ?
O11 Cu1 N15 93.29(14) . . ?
O11 Cu1 N2 88.84(15) . . ?
N15 Cu1 N2 166.97(17) . . ?
O11 Cu1 N18 174.01(15) . . ?
N15 Cu1 N18 84.82(15) . . ?
N2 Cu1 N18 91.75(15) . . ?
O11 Cu1 O100 96.52(13) . . ?
N15 Cu1 O100 97.55(14) . . ?
N2 Cu1 O100 94.97(15) . . ?
N18 Cu1 O100 89.37(14) . . ?
C2 Ni2 C2 180.00(16) . 3_566 ?
C2 Ni2 C1 88.5(2) . 3_566 ?
C2 Ni2 C1 91.5(2) 3_566 3_566 ?
C2 Ni2 C1 91.5(2) . . ?
C2 Ni2 C1 88.5(2) 3_566 . ?
C1 Ni2 C1 180.00(16) 3_566 . ?
C2 N2 Cu1 170.0(4) . . ?
C14 N15 C16 119.5(4) . . ?
C14 N15 Cu1 126.5(3) . . ?
C16 N15 Cu1 114.0(3) . . ?
C182 N18 C181 110.0(4) . . ?
C182 N18 C17 107.4(4) . . ?
C181 N18 C17 110.4(4) . . ?
C182 N18 Cu1 117.2(3) . . ?
C181 N18 Cu1 108.4(3) . . ?
C17 N18 Cu1 103.2(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.170(6) . ?
C1 Ni2 1.867(6) . ?
C2 N2 1.161(6) . ?
C2 Ni2 1.858(5) . ?
C12 O11 1.284(5) . ?
C12 C13 1.381(7) . ?
C12 C121 1.493(7) . ?
C13 C14 1.422(7) . ?
C13 H13 0.9300 . ?
C14 N15 1.302(6) . ?
C14 C141 1.510(6) . ?
C16 N15 1.483(6) . ?
C16 C17 1.504(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N18 1.502(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C121 H12A 0.9600 . ?
C121 H12B 0.9600 . ?
C121 H12C 0.9600 . ?
C141 H14A 0.9600 . ?
C141 H14B 0.9600 . ?
C141 H14C 0.9600 . ?
C181 N18 1.484(7) . ?
C181 H18A 0.9600 . ?
C181 H18B 0.9600 . ?
C181 H18C 0.9600 . ?
C182 N18 1.478(6) . ?
C182 H18D 0.9600 . ?
C182 H18E 0.9600 . ?
C182 H18F 0.9600 . ?
O11 Cu1 1.938(3) . ?
O100 Cu1 2.328(3) . ?
O100 H1 0.848(18) . ?
O100 H2 0.82(3) . ?
Cu1 N15 1.947(4) . ?
Cu1 N2 1.971(4) . ?
Cu1 N18 2.060(4) . ?
Ni2 C2 1.858(5) 3_566 ?
Ni2 C1 1.867(6) 3_566 ?
